CN105974060A - Method for detecting cobalt removal depth of polycrystalline diamond compact - Google Patents
Method for detecting cobalt removal depth of polycrystalline diamond compact Download PDFInfo
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- CN105974060A CN105974060A CN201610299980.9A CN201610299980A CN105974060A CN 105974060 A CN105974060 A CN 105974060A CN 201610299980 A CN201610299980 A CN 201610299980A CN 105974060 A CN105974060 A CN 105974060A
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- cobalt
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- depth
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- tangent plane
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
Abstract
The invention discloses a method for detecting cobalt removal depth of a polycrystalline diamond compact. The method comprises the following steps: pretreatment is carried out for the polycrystalline diamond compact with cobalt removed; the polycrystalline diamond compact is cut at a diameter direction along a cross section; further processing is carried out for a section of the polycrystalline diamond compact; scanning and screenshot are carried out for the section, and the cobalt removal depth is marked. The method for detecting cobalt removal depth of the polycrystalline diamond compact has a simplified flow for preparing a sample, so that detection cost is substantially reduced.
Description
Technical field
The invention belongs to sintered carbide tools manufacturing technology field, particularly relate to a kind of detection polycrystalline diamond multiple
Close the method that sheet takes off the cobalt degree of depth.
Background technology
Along with diamond compact is in extensively application and the oil-gas mining in the fields such as oil and natural gas exploitation
Improving constantly of technology, also grows with each passing day to the demand of high abrasion-proof diamond composite sheet.Diamond is combined
Sheet carries out de-cobalt operation can be effectively improved the heat resistance of product, thus greatly improves diamond compact
The wearability of product.
At present, it is applied to composite polycrystal-diamond and takes off the method for cobalt and mainly include electrolysis and the acid-hatching of young eggs,
Although principle difference, but can effectively dispel the existence of part cobalt in diamond layer, it is effectively improved
Heat-resisting and the anti-wear performance of diamond compact.In order to meet the demand of different levels client, complete at de-cobalt
Cheng Hou, needs to be measured the de-cobalt degree of depth.The most general de-cobalt degree of depth assay method mainly has two
Kind: one is to utilize Powerful Light Microscope or derivative determinator, it is possible to realize the rough survey of the de-cobalt degree of depth
Fixed, but reference value is not strong, and cogency is limited；Two is to utilize scanning electron microscope, can effectively realize
Diverse location difference takes off the accurate measurement of cobalt depths products, but needs in the preparation process of sample non-conductive
Position carries out metal spraying process, relatively costly, and flow process very complicated.
Summary of the invention
For solving above-mentioned technical problem, the invention provides a kind of detection composite polycrystal-diamond, to take off cobalt deep
The method of degree, it is possible to utilize the flow process simplified to prepare sample, and testing cost can be substantially reduced.
The a kind of of present invention offer detects the method that composite polycrystal-diamond takes off the cobalt degree of depth, including:
Composite polycrystal-diamond after de-cobalt is carried out pretreatment；
Described composite polycrystal-diamond is cut along diameter of section direction；
The tangent plane of described composite polycrystal-diamond is processed further；
Described tangent plane is scanned and sectional drawing the de-cobalt degree of depth is labeled.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described to de-cobalt
After composite polycrystal-diamond carry out pretreatment and include:
To cylindrical, the hard alloy end face of the composite polycrystal-diamond after de-cobalt and chamfering is processed,
Polishing and cleaning.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described to described
Composite polycrystal-diamond carries out cutting along diameter of section direction and includes:
Utilize high power laser light cutting machine from the end face of described composite polycrystal-diamond along diameter of section direction
Cut；
Utilize wire cutting machine from the bottom surface of described composite polycrystal-diamond along same described diameter of section side
To proceeding cutting.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described to described
The tangent plane of composite polycrystal-diamond is processed further including:
Utilize finishing fixture that described tangent plane is repaired；
Utilize one side pressurization mirror finishing machine or metallic phase polisher milling that described tangent plane is carried out at further polishing
Reason；
Utilize metal cleaner that described tangent plane is carried out pretreatment cleaning；
Utilize ultrasonic washing unit that described tangent plane is carried out ultrasonic cleaning；
Utilize drying baker that described tangent plane is dried.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described to described
Tangent plane was scanned before sectional drawing also including:
The enlargement ratio arranging scanning position is 100 times to 200 times.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described to de-cobalt
The degree of depth is labeled including:
Each position of scanning is carried out the mark at no less than two, and at least a part of which includes that the de-cobalt degree of depth is the highest
Point and de-cobalt degree of depth minimum point.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described to described
Tangent plane is scanned including with sectional drawing:
Described tangent plane is carried out six sectional drawings, described sectional drawing at least includes the non-cobalt layers in interface and the non-cobalt of chamfering
Layer.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, in described sectional drawing
Also include the non-cobalt layers of cylindrical.
Preferably, in above-mentioned detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described to described
Tangent plane is scanned also including with sectional drawing and after being labeled the de-cobalt degree of depth:
Arranging scanning enlargement ratio is 1000 times to 2000 times, is scanned cobalt containing layer and sectional drawing.
By foregoing description, the detection composite polycrystal-diamond that the present invention provides takes off the side of the cobalt degree of depth
Method, owing to first carrying out pretreatment, then to described glomerocryst Buddha's warrior attendant to the composite polycrystal-diamond after de-cobalt
Stone composite sheet is cut along diameter of section direction, then carries out the tangent plane of described composite polycrystal-diamond
It is processed further, then described tangent plane is scanned and sectional drawing the de-cobalt degree of depth is labeled, it is to avoid
Its surface is carried out metal spraying process, therefore, it is possible to utilize the flow process simplified to prepare sample, and can be big
Reduce greatly testing cost.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to reality
Execute the required accompanying drawing used in example or description of the prior art to be briefly described, it should be apparent that below,
Accompanying drawing in description is only embodiments of the invention, for those of ordinary skill in the art, not
On the premise of paying creative work, it is also possible to obtain other accompanying drawing according to the accompanying drawing provided.
Fig. 1 takes off the side of the cobalt degree of depth for the first detection composite polycrystal-diamond that the embodiment of the present application provides
The flow chart of method.
Detailed description of the invention
The core concept of the present invention is to provide a kind of composite polycrystal-diamond that detects to take off the side of the cobalt degree of depth
Method, it is possible to utilize the flow process simplified to prepare sample, and testing cost can be substantially reduced.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out
Clearly and completely describe, it is clear that described embodiment is only a part of embodiment of the present invention, and
It is not all, of embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under creative work premise, broadly fall into the scope of protection of the invention.
The first detection composite polycrystal-diamond that the embodiment of the present application provides takes off the method such as figure of the cobalt degree of depth
Shown in 1, the first detection composite polycrystal-diamond that Fig. 1 provides for the embodiment of the present application takes off the cobalt degree of depth
The flow chart of method.The method comprises the steps:
S1: the composite polycrystal-diamond after de-cobalt is carried out pretreatment；
In this step, the appearance being primarily directed to the composite polycrystal-diamond after de-cobalt processes,
Accomplish smooth in appearance and cleaning, to avoid impurity that detection is adversely affected.
S2: described composite polycrystal-diamond is cut along diameter of section direction；
In this step, by the composite polycrystal-diamond after de-cobalt along the diametric(al) of its circular cross section,
Down cutting, just expose whole tangent plane after cutting, this tangent plane just can show the de-cobalt at each position
Situation.
S3: the tangent plane of described composite polycrystal-diamond is processed further；
After cutting, the tangent plane obtained is the most coarse, it is impossible to directly apply to scanning electron microscope detection,
It is thus desirable to it is for further processing to it, to obtain the pure tangent plane of flat smooth.
S4: described tangent plane is scanned and sectional drawing the de-cobalt degree of depth is labeled.
In this step, after obtaining the scanogram of described tangent plane, carry out sectional drawing, in the sectional drawing obtained,
Brighter owing to there is the position of cobalt element, and the position after de-cobalt is dark, therefore according to this bright dark
Difference just can distinguish de-cobalt layers and non-de-cobalt layers, utilizes this principle just can detect the de-cobalt degree of depth.
By foregoing description, the above-mentioned detection composite polycrystal-diamond that the embodiment of the present application provides takes off
The method of the cobalt degree of depth, owing to first carrying out pretreatment to the composite polycrystal-diamond after de-cobalt, then to institute
State composite polycrystal-diamond to cut along diameter of section direction, then to described composite polycrystal-diamond
Tangent plane be processed further, then described tangent plane is scanned and sectional drawing the de-cobalt degree of depth is carried out
Mark, it is to avoid its surface carried out metal spraying process, therefore, it is possible to utilize the flow process simplified to prepare sample,
And testing cost can be substantially reduced.
The method that the second detection composite polycrystal-diamond that the application provides takes off the cobalt degree of depth, is above-mentioned
On the basis of first method, also include following technical characteristic:
Described composite polycrystal-diamond after de-cobalt carried out pretreatment include:
To cylindrical, the hard alloy end face of the composite polycrystal-diamond after de-cobalt and chamfering is processed,
Polishing and cleaning.
It is said that in general, cut according to the overall height of composite polycrystal-diamond and the maximum of laser cutting machine
The degree of depth, possibly cannot disposably cut through whole composite polycrystal-diamond, therefore need after cut,
After same position is demarcated bottom composite polycrystal-diamond, cutting on line equipment carries out secondary cut,
Therefore, this application provides the method that the third detection composite polycrystal-diamond takes off the cobalt degree of depth, be upper
On the basis of stating second method, also include following technical characteristic:
Described described composite polycrystal-diamond carried out cutting along diameter of section direction include:
Utilize high power laser light cutting machine from the end face of described composite polycrystal-diamond along diameter of section direction
Cut；
Utilize wire cutting machine from the bottom surface of described composite polycrystal-diamond along same described diameter of section side
To proceeding cutting.
Concrete operating process is as follows: be first loaded on cutting clamper by composite polycrystal-diamond, with swashing
The composite bed of composite polycrystal-diamond is cut by light cutting machine, cuts complete turnover fixture, firmly
Demarcating according still further to diameter of section direction on matter alloy end face, such wire cutting machine is to cutter when, directly
Just can be with fully penetrated whole composite sheet along the line wire demarcated, and tangent plane is almost completely superposed, and tangent plane is relatively
Smooth.
The method that the 4th kind of detection composite polycrystal-diamond that the application provides takes off the cobalt degree of depth, is above-mentioned
On the basis of the third method, also include following technical characteristic:
The described tangent plane to described composite polycrystal-diamond is processed further including:
Utilize finishing fixture that described tangent plane is repaired；
Utilize one side pressurization mirror finishing machine or metallic phase polisher milling that described tangent plane is carried out at further polishing
Reason, concrete, the diamond layer end face of sample is loaded in special fixture down, is placed on one side pressurization
Mirror finishing machine or metallic phase polisher milling are polished, until interface occurs that bright luster just stops polishing；
Utilize metal cleaner that described tangent plane is carried out pretreatment cleaning；
Utilize ultrasonic washing unit that described tangent plane is carried out ultrasonic cleaning, concrete, it is possible to use anhydrous second
Alcohol is medium, cleans sample 10 minutes with ultrasonic washing unit；
Utilize drying baker that described tangent plane is dried, concrete, can dry at 80 DEG C with drying baker,
Naturally cool to room temperature take out to be placed in sealing bag and seal up for safekeeping and number, identify, in case censorship.
The method that the 5th kind of detection composite polycrystal-diamond that the application provides takes off the cobalt degree of depth, is above-mentioned
On the basis of 4th kind of method, also include following technical characteristic:
Described described tangent plane be scanned and also include before sectional drawing:
The enlargement ratio arranging scanning position is 100 times to 200 times.
It is to say, de-cobalt depth detection all scanning position enlargement ratio is 100-200X, weight after sectional drawing
New name (cobalt layers 01 as non-in interface, non-cobalt layers of the non-cobalt layers in interface 02 or interface 03 etc.), outside containing
Circle, chamfering and interface take off cobalt layers.
The method that the 6th kind of detection composite polycrystal-diamond that the application provides takes off the cobalt degree of depth, is above-mentioned
On the basis of fifth method, also include following technical characteristic:
Described it is labeled including to the de-cobalt degree of depth:
Each position of scanning is carried out the mark at no less than two, and at least a part of which includes that the de-cobalt degree of depth is the highest
Point and de-cobalt degree of depth minimum point.
In this case, it becomes possible to position that the de-cobalt degree of depth of record is the highest and minimum position, it is thus possible to
Enough overall situations to the de-cobalt degree of depth are held.
The method that the 7th kind of detection composite polycrystal-diamond that the application provides takes off the cobalt degree of depth, is above-mentioned
On the basis of 6th kind of method, also include following technical characteristic:
Described described tangent plane is scanned and sectional drawing includes:
Described tangent plane is carried out six sectional drawings, described sectional drawing at least includes the non-cobalt layers in interface and the non-cobalt of chamfering
Layer.
Concrete, diamond layer interface divides three sections of lines to sweep, and contains whole diamond layer interface, and sectional drawing amounts to 3
?；Up and down or left and right chamfering non-cobalt layers overall picture and interface non-cobalt layers local the most all in same sectional drawing show, section
Figure amounts to 2；Further, described sectional drawing can also include the non-cobalt layers of cylindrical.
It addition, in any of the above-described kind of detection composite polycrystal-diamond takes off the method for the cobalt degree of depth, described right
Described tangent plane is scanned can also preferably including with sectional drawing and after being labeled the de-cobalt degree of depth:
Arranging scanning enlargement ratio is 1000 times to 2000 times, is scanned cobalt containing layer and sectional drawing, so
How the cobalt being known that in diamond layer is distributed, thus plays certain guidance work to producing and researching and developing
With.
Below concrete sample detection step is described below: sample is placed on sample stage, uses conducting resinl
Viscous sample is fixed, and closes sample switch room door, and evacuation processes, and after specified vacuum degree to be achieved, regulation sets
Standby and parameter, after reaching predetermined state, regulation amplification, focal length, brightness, contrast, astigmatism etc.,
Obtain picture rich in detail, carry out sample detection.
Criterion for the de-cobalt degree of depth is as described below:
Different according to the de-cobalt degree of depth, de-cobalt mode is defined as: shallow de-cobalt, deep de-cobalt and ultra-deep take off cobalt three
Kind, above-mentioned three kinds of de-cobalts also can be coordinated to carry out for the side of the non-cobalt layers of cylindrical and to process.
The criterion of the different de-cobalt degree of depth is as follows:
Shallow de-cobalt, its de-cobalt degree of depth is 150-250 μm, and cylindrical non-cobalt layers height is more than 250 μm；
Deep de-cobalt, its de-cobalt degree of depth is 250-500 μm, and cylindrical non-cobalt layers height is more than 250 μm；
Ultra-deep takes off cobalt, and its de-cobalt degree of depth is more than 500 μm, and cylindrical non-cobalt layers height is more than 250 μm.
It should be noted that the scope of the de-cobalt degree of depth should include whole diamond layer and cover whole chamfering,
The process degree of depth of chamfering should keep consistent with the process degree of depth of plane, and whole de-cobalt layers should be from diamond layer
Center is arrived to edge again should keep relatively uniform smooth at chamfering, and depth capacity difference is not to be exceeded 100 microns.
This just specify that testing process and the method utilizing the de-cobalt of scanning electron microscope detection, and defines concrete judgement
Standard, makes detection more standardized and orderly.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses
The present invention.Multiple amendment to these embodiments will be aobvious and easy for those skilled in the art
See, generic principles defined herein can without departing from the spirit or scope of the present invention,
Realize in other embodiments.Therefore, the present invention is not intended to be limited to the embodiments shown herein,
And it is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (9)
1. one kind is detected the method that composite polycrystal-diamond takes off the cobalt degree of depth, it is characterised in that including:
Composite polycrystal-diamond after de-cobalt is carried out pretreatment；
Described composite polycrystal-diamond is cut along diameter of section direction；
The tangent plane of described composite polycrystal-diamond is processed further；
Described tangent plane is scanned and sectional drawing the de-cobalt degree of depth is labeled.
The method that detection composite polycrystal-diamond the most according to claim 1 takes off the cobalt degree of depth, it is special
Levy and be, described composite polycrystal-diamond after de-cobalt is carried out pretreatment include:
To cylindrical, the hard alloy end face of the composite polycrystal-diamond after de-cobalt and chamfering is processed,
Polishing and cleaning.
The method that detection composite polycrystal-diamond the most according to claim 2 takes off the cobalt degree of depth, it is special
Levy and be, described described composite polycrystal-diamond is carried out cutting along diameter of section direction include:
Utilize high power laser light cutting machine from the end face of described composite polycrystal-diamond along diameter of section direction
Cut；
Utilize wire cutting machine from the bottom surface of described composite polycrystal-diamond along same described diameter of section side
To proceeding cutting.
The method that detection composite polycrystal-diamond the most according to claim 3 takes off the cobalt degree of depth, it is special
Levying and be, the described tangent plane to described composite polycrystal-diamond is processed further including:
Utilize finishing fixture that described tangent plane is repaired；
Utilize one side pressurization mirror finishing machine or metallic phase polisher milling that described tangent plane is carried out at further polishing
Reason；
Utilize metal cleaner that described tangent plane is carried out pretreatment cleaning；
Utilize ultrasonic washing unit that described tangent plane is carried out ultrasonic cleaning；
Utilize drying baker that described tangent plane is dried.
The method that detection composite polycrystal-diamond the most according to claim 4 takes off the cobalt degree of depth, it is special
Levy and be, described described tangent plane be scanned and also include before sectional drawing:
The enlargement ratio arranging scanning position is 100 times to 200 times.
The method that detection composite polycrystal-diamond the most according to claim 5 takes off the cobalt degree of depth, it is special
Levy and be, described be labeled including to the de-cobalt degree of depth:
Each position of scanning is carried out the mark at no less than two, and at least a part of which includes that the de-cobalt degree of depth is the highest
Point and de-cobalt degree of depth minimum point.
The method that detection composite polycrystal-diamond the most according to claim 6 takes off the cobalt degree of depth, it is special
Levy and be, described described tangent plane is scanned and sectional drawing includes:
Described tangent plane is carried out six sectional drawings, described sectional drawing at least includes the non-cobalt layers in interface and the non-cobalt of chamfering
Layer.
The method that detection composite polycrystal-diamond the most according to claim 7 takes off the cobalt degree of depth, it is special
Levy and be, described sectional drawing also includes the non-cobalt layers of cylindrical.
9. the side of the cobalt degree of depth is taken off according to the detection composite polycrystal-diamond described in any one of claim 1-8
Method, it is characterised in that described described tangent plane is scanned and sectional drawing the de-cobalt degree of depth is labeled it
After also include:
Arranging scanning enlargement ratio is 1000 times to 2000 times, is scanned cobalt containing layer and sectional drawing.
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| CN108318538A (en) * | 2018-03-08 | 2018-07-24 | 苏州思珀利尔工业技术有限公司 | Detect the device and method that composite polycrystal-diamond takes off cobalt depth |
| CN108663312A (en) * | 2018-03-08 | 2018-10-16 | 苏州思珀利尔工业技术有限公司 | The method for taking off cobalt depth is detected based on wire cutting |
| WO2018205497A1 (en) * | 2017-05-09 | 2018-11-15 | 河南四方达超硬材料股份有限公司 | Cobalt-removed polycrystalline diamond compact |
| CN110470200A (en) * | 2019-09-02 | 2019-11-19 | 武汉锐特金刚石有限公司 | A method of detection diamond compact takes off cobalt depth |
| CN111911082A (en) * | 2020-07-11 | 2020-11-10 | 长江大学 | Method for strengthening polycrystalline diamond compact |
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| CN107085002A (en) * | 2017-04-24 | 2017-08-22 | 河南四方达超硬材料股份有限公司 | A kind of high temperature resistant wire drawing die takes off the lossless detection method of cobalt depth |
| CN107085002B (en) * | 2017-04-24 | 2019-12-24 | 河南四方达超硬材料股份有限公司 | Nondestructive testing method for cobalt removal depth of high-temperature-resistant wire-drawing die |
| WO2018205497A1 (en) * | 2017-05-09 | 2018-11-15 | 河南四方达超硬材料股份有限公司 | Cobalt-removed polycrystalline diamond compact |
| CN108318538A (en) * | 2018-03-08 | 2018-07-24 | 苏州思珀利尔工业技术有限公司 | Detect the device and method that composite polycrystal-diamond takes off cobalt depth |
| CN108663312A (en) * | 2018-03-08 | 2018-10-16 | 苏州思珀利尔工业技术有限公司 | The method for taking off cobalt depth is detected based on wire cutting |
| CN110470200A (en) * | 2019-09-02 | 2019-11-19 | 武汉锐特金刚石有限公司 | A method of detection diamond compact takes off cobalt depth |
| CN110470200B (en) * | 2019-09-02 | 2024-02-20 | 武汉锐特金刚石有限公司 | Method for detecting cobalt removal depth of diamond compact |
| CN111911082A (en) * | 2020-07-11 | 2020-11-10 | 长江大学 | Method for strengthening polycrystalline diamond compact |
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